Magnetic separation has been proved to be superior to the traditional column separation or filtration especially when nanosized adsorbents are used. In this work, iron phosphate coated nano-Fe3O4 particles (Fe3O4@FePO4) were synthesized in aqueous solution through deposition of Fe(III) and phosphate ions onto the superparamagnetic nano-Fe3O4 particles that were prepared by coprecipitation. The synthesized nano-particles were applied to the enrichment of trace amounts of Cr(III) for its determination by graphite furnace atomic absorption spectrometry (GF-AAS). The magnetic property and morphology of Fe3O4@FePO4 were characterized by vibrating sample magnetometer (VSM), scanning electron microscope (SEM), transmission electron microscope (TEM). The results indicated that the adsorbent was superparamagnetic. Its saturated intensity of magnetization was 23.0 emu•g-1. This value implied that the prepared Fe3O4@FePO4 could be efficiently separated from the solutions by magnetic fields. The diameters of the particles evaluated from TEM images were in a range of 2～9 nm, which were consistent with that obtained from dynamic light scattering. X-ray photoelectron spectroscopy (XPS) and Zeta potential measurement were used for determining the composition and surface charge of the adsorbent. Based on XPS results, the amount of FePO4 in Fe3O4@FePO4 was 33.8%. Cr was found in Fe3O4@FePO4 after Cr adsorption. Zeta potential measurement indicated that the surface of Fe3O4@FePO4 carried positive charge at pH<4 and negative charge at pH>4. The influence of pH, adsorption time and sample volume on the rate of adsorption were systematically investigated. At pH 5.3, 0.0200 g of Fe3O4@FePO4 could quantitatively adsorb Cr(III) from 20.0 mL of sample within 20 min. Freundlich isotherm and pseudo second order adsorption kinetics were observed. Adsorbed Cr(III) could be desorbed with 0.3 mol•L-1 NH3-1% (V/V) H2O2 for direct GF-AAS analysis. The adsorbent was also used for the enrichment of Cr(III) from large volume samples. After stirring for 2 h, more than 80% of Cr(III) in 800 mL (0.5 μg•L-1) of aqueous solution could be adsorbed and an enrichment factor of 1125 was attained, which confirmed its suitability for the analysis of trace amounts of Cr(III). The adsorbent was successfully used for the real sample analysis and could be re-used 10 times after proper washing and drying.
王都留, 杨建东, 杨升宏, 郭锦秀. FePO4包覆Fe3O4磁性纳米微粒的合成及其在Cr(III)富集分离中的应用[J]. 化学学报, 2013, 71(09): 1287-1292.
Wang Duliu, Yang Jiandong, Yang Shenghong, Guo Jinxiu. Synthesis of Iron Phosphate Coated Nano-Fe3O4 Particles and Its Application in the Enrichment of Chromium(III) from Aqueous Solutions. Acta Chimica Sinica, 2013, 71(09): 1287-1292.